Reference of 194853-86-6,Some common heterocyclic compound, 194853-86-6, name is 4-Fluoro-2-(trifluoromethyl)benzonitrile, molecular formula is C8H3F4N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A.7V-[4-cyano-3-(trifluoromethyl)phenyl]-D-valineA mixture of 4-fluoro-2-(trifluoromethyl)benzonitrile (reagent A) (500 mg, 2.64 mmol, 1 eq), D- valine (reagent B) (341 mg, 2.91 mmol, 1.1 eq), and K2CO3 (547 mg, 3.96 mmol, 1.5 eq) in DMF (6 mL) was sealed in a 10-20 mL microwave process vial and heated in a microwave reactor for 20 min at 100 0C. The reaction mixture was partitioned between ethyl acetate and water and acidified to pH 3 with IN HCl. The layers were separated, and the organic layer was washed with saturated aqueous sodium carbonate (2-50 mL portions) and dried over sodium sulfate. The residue was purified by ISCO silica gel chromatography (1Og silica cartridge, 100% CH2Cl2 grading to 10% CH3OH/CH2C12 over 10 min followed by 10% CH2Cl2 for 10 min) to provide the title compound (320 mg, 42%) as a pale yellow oil. 1H NMR (400 MHz, CD3OD) delta 7.63 (d, IH, J = 8.8 Hz), 7.13 (d, IH, J= 2.0 Hz), 6.88 (dd, IH, J = 8.4, 2.0 Hz), 3.91 (d, IH, 7= 6.4 Hz), 2.24 (m, IH), 1.09 (t, 6H, J = 6.8 Hz); LC/MS 287.2 (MH)+.
The synthetic route of 194853-86-6 has been constantly updated, and we look forward to future research findings.